Learning objectives
The course aims to provide students with advanced knowledge of the
analytical process, the classification of analytical methods and the main
instrumental analytical techniques, with particular regard to
spectroscopic, separative and coupled analytical techniques. A critical
discussion of the principles, performance and fields of applicability of the
techniques is emphasized. The aim of the course is also to guide students
to a critical evaluation of the experimental results in relation to the
performance of instrumental techniques, the field of investigation
(qualitative, quantitative or confirmation method) and to the quality
parameters of the analytical methods, applying a "problem solving"
approach. The concept of validation of analytical methods is defined and
the European guidelines for validation are illustrated.
At the end of the course the student is expected to be able to:
- know the principles and the analysis procedures for the characterization
of chemical compounds;
- to know the fundamental principles of the methods of instrumental
analysis, with the classification of the instrumental analytical techniques,
and the relative selection criteria;
- performing stoichiometric calculations and practical operations in
relation to the preparation of solutions of known concentration;
- choose and use the best method of separation, purification and analysis
of a mixture;
- collect scientific data through laboratory observations and
measurements, to elaborate and interpret them;
- carry out the sampling, the preparation of the sample and draw up the
documentation of the analysis performed;
- communicate, both in oral and written form, in the context of
professional activities and relationships, with a strict respect for the
chemical language;
- interacting with other staff on the implementation of procedures and the
necessary safety measures in the chemical field;
- undertake academic studies of a higher level with a sufficient degree of
autonomy or to continue the professional training;
- work by objectives, in groups or independently;
- adapt to different areas of work and issues;
- to interpret, in an autonomous way, data of technical-scientific
literature, especially in the practical-applicative field
Prerequisites
Physics I. Physics II.
Analytical Chemistry and Laboratory of Analytical Chemistry.
Analytical Chemistry II and Chemometrics
Course unit content
Introduction to instrumental analytical methods
Classification of analytical techniques
Criteria for the choice of analytical methods. Development and validation
of analytical methods.
Method performance characteristics.
Calibration methods.
Spectroscopic techniques
Molecular Absorption and Fluorescence UV-vis Spectrophotometry.
Molecular Absorption IR Spectrophotometry.
Atomic Absorption Spectrophotometry.
Atomic Emission Spectrophotometry.
Mass Spectrometry.
X-ray Diffraction.
Separation techniques
Theory and application of chromatography. Gas chromatography and
liquid chromatography.
Laboratory experiments
Full programme
Introduction to instrumental analytical methods
Classification of analytical techniques
Criteria for the choice of analytical methods. Development and validation
of analytical methods.
Method performance characteristics according to European guidelines for
the validation of analytical methods: linearity range, detection and
quantitation limits, sensitivity, selectivity, accuracy (precision and
trueness).
Types of calibration methods: external calibration, internal
standardization, standard addition method.
Spectroscopic techniques
Fundamentals of spectrophotometry.
Molecular Absorption and Fluorescence UV-vis Spectrophotometry. The
nature of electronic transitions. Instrumentation for molecular absorption
UV-vis spectrophotometry: sources, monochromators, detectors.
Photodiode array detector. Trasmittance and absorbance. Lambert-Beer
law and deviations. Applications to quantitative analysis.
Instrumentation for molecular fluorescence UV-vis spectrophotometry.
Fluorescence and phosphorescence. Effect of temperature on the
fluorescence quantum yield. Quantitation: relation between the intensity
of fluorescence emission of dilute samples and analyte concentration.
Atomic Absorption Spectrophotometry. Atomic spectra. Instrumentation:
hollow cathod lamp, atomizers (flame and graphite furnace atomic
absorption spectroscopy, hydride generation atomic absorption
spectroscopy, Cold vapor atomic absorption spectroscopy). Spectral and
non spectral interferences. Background correction systems.
Atomic Emission Spectrophotometry. Instrumentation: ICP source, high resolution
monochromators, detectors.
Molecular Absorption IR Spectrophotometry. Modes of molecular motion;
vibrational modes and absorption regions. Factors that influence the
frequency of absorption. Characteristic IR absorption frequencies. FT-IR
instrumentation: sources, Michelson interferometer, detectors. FT-IR gas
analysis. Applications of IR spectroscopy to the characterization of
organic compounds.
Mass Spectrometry. Fundamentals. Instrumentation: electron ionization
source, chemical ionization source, analyzers (magnetic sector,
quadrupoles, ion trap, time-of-flight), detector.
X-ray Diffraction. Fundamentals and instrumentation.
Separation techniques
Theory and application of chromatography. Gas chromatography and
liquid chromatography.
Chromatographic parameters. Retention time. Capacity factor. Selectivity
factor. Resolution. Band broadening and column efficiency.
Gas chromatography. Gas-solid chromatography (GSC). Gas-liquid
chromatography (GLC). Stationary phases for GSC and GLC.
Instrumentation: injectors, columns, detectors. Capillary columns.
Universal and selective detectors. Gas chromatography-mass
spectrometry. Isothermal gas chromatography. Temperatureprogrammed
gas chromatography. Internal standard calibration method
for quantitative determinations.
Liquid chromatography (TLC, preparative LC and analytical LC (HPLC)).
Mechanisms of separation: adsorption chromatography, partition
chromatography, ion chromatography, size-exclusion chromatography.
Instrumentation for HPLC: injection valve, columns, pumps, detectors.
Isocratic elution, gradient elution.Applications to quantitative analysis.
Instrumentation for molecular fluorescence UV-vis spectrophotometry. Fluorescence and phosphorescence. Effect of temperature on the fluorescence quantum yield. Quantitation: relation between the intensity of fluorescence emission of dilute samples and analyte concentration.
Atomic Absorption Spectrophotometry. Atomic spectra. Instrumentation: hollow cathod lamp, atomizers (flame and graphite furnace atomic absorption spectroscopy, hydride generation atomic absorption spectroscopy, Cold vapor atomic absorption spectroscopy). Spectral and non spectral interferences. Background correction systems.
Atomic Emission Spectrophotometry. Instrumentation: ICP source, high-resolution monochromators, detectors.
Molecular Absorption IR Spectrophotometry. Modes of molecular motion; vibrational modes and absorption regions. Factors that influence the frequency of absorption. Characteristic IR absorption frequencies. FT-IR instrumentation: sources, Michelson interferometer, detectors. FT-IR gas analysis. Applications of IR spectroscopy to the characterization of organic compounds.
Mass Spectrometry. Fundamentals. Instrumentation: electron ionization source, chemical ionization source, analyzers (magnetic sector, quadrupoles, ion trap, time-of-flight), detector.
X-ray Diffraction. Fundamentals and instrumentation.
Separation techniques
Theory and application of chromatography. Gas chromatography and liquid chromatography.
Chromatographic parameters. Retention time. Capacity factor. Selectivity factor. Resolution. Band broadening and column efficiency.
Gas chromatography. Gas-solid chromatography (GSC). Gas-liquid chromatography (GLC). Stationary phases for GSC and GLC. Instrumentation: injectors, columns, detectors. Capillary columns. Universal and selective detectors. Gas chromatography-mass spectrometry. Isothermal gas chromatography. Temperature-programmed gas chromatography. Internal standard calibration method for quantitative determinations.
Liquid chromatography (TLC, preparative LC and analytical LC (HPLC)). Mechanisms of separation: adsorption chromatography, partition chromatography, ion chromatography, size-exclusion chromatography. Instrumentation for HPLC: injection valve, columns, pumps, detectors. Isocratic elution, gradient elution.
Bibliography
K.A. Rubinson, J.F. Rubinson, Chimica Analitica Strumentale, Zanichelli,
2002.
Holler, Skoog, Crouch, Chimica Analitica Strumentale, II edizione, EdiSES,
2009.
D.S. Hage, J.D. Carr, Chimica Analitica e Analisi Quantitativa, Piccin, 2012.
Teaching methods
Academic teaching. Interactive teaching. Laboratory experiments.
Academic teaching will be supported by interactive educational paths
with the aim of stimulating interest in the subject and comparing
different approaches to the topics covered.
Cycles of analytical laboratory experiences will be activated for 1 CFU (15
hours) during which students will be required to apply the most relevant
analytical techniques according to the methodological criteria illustrated
in the lessons. For each laboratory experience the student will be
required to prepare a hand written report with a discussion of the analytical results.
The teaching materials used in the classroom are uploaded to Elly at the
beginning of the course. The slides of the Course are considered an
integral part of the teaching material.
Assessment methods and criteria
The acquired knowledge i.e. learning of the basic concepts and tools of instrumental analytical chemistry, acquisition of a formally correct language, ability to express
contents in a clear and linear way, elaboration of links between the different parts of the course. Critical evaluation of instrumental analytical techniques and correct classification of analytical methods, critical evaluation of the quality parameters of the methods, and the ability to understand the concepts treated are verified through a written and oral examination.
The written test, with an open answer, has a duration of 2 hours. The
written test is evaluated with a scale from very poor to excellent. The written examination is preclusive of the oral one an if the score is consecutively 2 times very poor the student must have a call with the teacher before the next trial. The result of the written test
is published within two days following the test.
In the oral examination, the student is evaluated on the basic concepts of
instrumental analytical chemistry, on the acquisition of a formally correct
language, and on the definition of relationships between the different
parts of the course. A critical evaluation of instrumental analytical
techniques and a correct classification of analytical methods is also
required, with a critical evaluation of the quality parameters of the
methods. The activity carried out in the laboratory will also be examined
through an assessment of the lab report and through learning of the
concepts related to the experiments. The lab report is to be delivered at least ten days before the date of the oral exam; please note that the last deadline for the report delivery is 28th February of the course attendance year, also in case of enrollment to subsequent exam sessions. The final evaluation (scale 0-30) is communicated immediately at the end of the oral test taking in account the oral examination itself, the written test result and the laboratory activity.
Please note that online registration is mandatory both in the case of a
written test and in the case of an oral exam.
Other information
Illustration of case studies of instrumental analytical techniques in the
food, environmental, biological and forensic fields.
